QuEChERS结合一次性滴管辅助的分散液液微萃取快速测定蔬菜中7种拟除虫菊酯类农药  

Rapid determination of seven pyrethroid pesticides in vegetables by combining QuEChERS with disposable polyethylene pipet assisted dispersed liquid-liquid micro extraction

作　　者：杨进劼 乐诗文 覃胜 赵琴 YANG Jinjie;YUE Shiwen;QIN Sheng;ZHAO Qin(School of Public Health,Wuhan University of Science and Technology,Hubei Provincial Key Laboratory of Occupational Hazard Identification and Control,Hubei Wuhan 430065,China;Center For Disease Control of Yiling District,Hubei Province,Hubei Yichang,443100,China)

机构地区：[1]武汉科技大学公共卫生学院,职业危害识别与控制湖北省重点实验室,湖北武汉430065 [2]湖北省宜昌市夷陵区疾病预防控制中心,湖北宜昌443100

出　　处：《中国食品卫生杂志》2024年第10期1130-1137,共8页Chinese Journal of Food Hygiene

摘　　要：目的将QuEChERS与一次性滴管辅助的分散液液微萃取(DPP-DLLME)技术联用,结合GC-ECD检测,建立一种可同时检测蔬菜中7种拟除虫菊酯类农药的新方法。方法首先使用乙腈作为提取剂对匀质蔬菜样品中的拟除虫菊酯类农药进行提取,收集的乙腈提取液经QuEChERS净化后作为DPP-DLLME的分散剂,采用一次性滴管为萃取容器,正辛醇为萃取剂,萃取完成后,萃取剂聚集漂浮在一次性滴管上端的窄颈处,直接提取进样。考察富集效率的影响因素,优化提取液的种类和作为分散剂时的用量、萃取剂的种类和体积、离子强度等一系列参数。结果在优化的萃取条件下,7种拟除虫菊酯类农药在0.5~200 ng/g范围内有良好的线性关系,r^(2)大于0.995,检出限在0.04~0.1 ng/g之间,定量限在0.1~0.5 ng/g之间。低中高三个浓度(1、10、100 ng/g)的加标回收率在94.5%~110.5%之间,日内日间相对标准差分别小于9.0%、8.2%。结论该方法前处理操作简单,除杂效果好,富集效率高,同时具有经济性和环保性,为蔬菜中拟除虫菊酯类农药检测提供了新方法。Objective A new method for the separation and enrichment of pyrethroid pesticides in vegetables was developed by combining QuEChERS with disposable polyethylene pipet assisted dispersed liquid-liquid micro-extraction(DPP-DLLME).Methods Firstly,acetonitrile was used as extraction agent for separation of pyrethroid pesticides from vegetable samples,and the collected acetonitrile extract was purified,then used as the dispersant of DPP-DLLME.A disposable dropper was used as the extraction vessel for DPP-DLLME,and n-octanol was used as the extractant.After phase separation,the extractant was floating on the aqueous solution and concentrated in the narrow neck of the pipet,which can be directly withdrawn by a microsyringe for instrument analysis.Results Under the optimized extraction conditions,the linearity range was 0.5-200 ng/g with correlation coefficient r^(2) higher than 0.995 for seven pyrethroid pesticides.The limits of detection were in the range of 0.04-0.1 ng/g,and the limits of quantitation were in the range of 0.1-0.5 ng/g.The recoveries at three spiking levels of 1,10 and 100 ng/g were in the range of 94.5%-110.5%with the RSDs less than 9.0%(intra-day)and 8.2%(inter-day).Conclusion The method was simple and effective,which provided a new choice for the detection of pyrethroid pesticides in vegetables.

关 键 词：QUECHERS 一次性滴管辅助的分散液液微萃取 拟除虫菊酯类农药 气相色谱法 蔬菜 农药残留 

分 类 号：R155[医药卫生—营养与食品卫生学]